ENGINEERING TRANSACTIONS • Engng. Trans. • 61, 3, 197–218, 2013 Polish Academy of Sciences • Institute of Fundamental Technological Research (IPPT PAN) National Engineering School of Metz (ENIM) The Structure Analysis of Secondary (Recycled) AlSi9Cu3 Cast Alloy with and without Heat Treatment Lenka HURTALOV ´ A, Eva TILLOV ´ A, M´ aria CHALUPOV ´ A University of ˇ Zilina Faculty of Mechanical Engineering, Department of Material Engineering Univerzitn´ a 1, 010 26 ˇ Zilina, Slovakia e-mail: [email protected]Al-Si alloys are very universal materials, comprising of from 85% to 90% of the aluminium cast parts produced for the automotive industry (e.g. various motor mounts, engine parts, cylinder heads, pistons, valve retainer, compressor parts, etc.). Production of primary Al- alloys belong to heavy source fouling of life environs. Care of environment of aluminium is connected to the decreasing consumption of resource as energy, materials, water, and soil, and with an increase in recycling and extension life of products in industry. Recycled (secondary) aluminium alloys are made out of Al-scrap and workable Al-garbage by recycling. The automotive casts from aluminium alloys are heat treated for achieving better properties. Al-Si alloys contain more addition elements, that form various intermetallic phases in the structure. They usually contain a certain amount of Fe, Mn, Mg, and Zn that are present either unintentionally, or they are added deliberately to provide special material properties. These elements partly go into the solid solution in the matrix and partly form intermetallic particles during solidification which affect the mechanical properties. Controlling the microstructure of secondary aluminium cast alloy is therefore very important. Key words: secondary Al alloy, intermetallic phases, structural analysis, solution treatment, mechanical properties. 1. Introduction The characteristic properties of aluminium, good formability, good corrosion resistance, high strength stiffness to weight ratio, and recycling possibilities make it as the ideal material to replace heavier materials (steel, cast iron or copper) in the car [1]. More than half aluminium on the present produce in European Union comes from recycled raw material. The primary aluminium production needs a lot of energy and constraints decision mining of bauxite. The European Union has big interest of share recycling aluminium and therefore increases interest about secondary aluminium alloys and cast stock from them [2].
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ENGINEERING TRANSACTIONS • Engng. Trans. • 61, 3, 197–218, 2013Polish Academy of Sciences • Institute of Fundamental Technological Research (IPPT PAN)
National Engineering School of Metz (ENIM)
The Structure Analysis of Secondary (Recycled) AlSi9Cu3Cast Alloy with and without Heat Treatment
Lenka HURTALOVA, Eva TILLOVA, Maria CHALUPOVA
University of ZilinaFaculty of Mechanical Engineering, Department of Material Engineering
Al-Si alloys are very universal materials, comprising of from 85% to 90% of the aluminiumcast parts produced for the automotive industry (e.g. various motor mounts, engine parts,cylinder heads, pistons, valve retainer, compressor parts, etc.). Production of primary Al- alloysbelong to heavy source fouling of life environs. Care of environment of aluminium is connectedto the decreasing consumption of resource as energy, materials, water, and soil, and with anincrease in recycling and extension life of products in industry. Recycled (secondary) aluminiumalloys are made out of Al-scrap and workable Al-garbage by recycling. The automotive castsfrom aluminium alloys are heat treated for achieving better properties. Al-Si alloys containmore addition elements, that form various intermetallic phases in the structure. They usuallycontain a certain amount of Fe, Mn, Mg, and Zn that are present either unintentionally, or theyare added deliberately to provide special material properties. These elements partly go into thesolid solution in the matrix and partly form intermetallic particles during solidification whichaffect the mechanical properties. Controlling the microstructure of secondary aluminium castalloy is therefore very important.
The characteristic properties of aluminium, good formability, good corrosionresistance, high strength stiffness to weight ratio, and recycling possibilities makeit as the ideal material to replace heavier materials (steel, cast iron or copper) inthe car [1]. More than half aluminium on the present produce in European Unioncomes from recycled raw material. The primary aluminium production needs alot of energy and constraints decision mining of bauxite. The European Unionhas big interest of share recycling aluminium and therefore increases interestabout secondary aluminium alloys and cast stock from them [2].
198 L. HURTALOVA, E. TILLOVA, M. CHALUPOVA
The replacement of primary aluminium with recycled has in recent years in-
creasing tendency. The recycled metal is a positive trend, because secondary alu-
minium produced from recycled metal requires only about 2.8 kWh/kg of metal
produced while primary aluminium production requires about 45 kWh/kg pro-
duced. The remelting of recycled metal saves almost 95% of the energy needed to
produce primary aluminium from ore, and, thus, triggers associated reductions
in pollution and greenhouse emissions from mining, ore refining, and melting.
Increasing the use of recycled metal is also quite important from an ecological
standpoint, since producing Al by recycling creates only about 5% as much CO2
as by primary production [3].
Due to the increasing utilization of recycled aluminium cast alloys, the qual-
ity of recycled Al-Si casting alloys is considered to be a key factor in selecting an
alloy casting for a particular engineering application. The mechanical properties
will be radically increasing by implementing adaptable alloying- and process
technology, leading to larger application fields of complex cast aluminium com-
ponents such as safety details. Generally, the mechanical and microstructural
properties of aluminium cast alloys are dependent on the composition; melt
treatment conditions, solidification rate, casting process and the applied thermal
treatment [4, 5]. The mechanical properties of Al-Si alloys depend, besides the
Si, Cu, Mg and Fe-content, more on the distribution and the shape of the silicon
particles [6]. The presence of additional elements in the Al-Si alloys allows many
complex intermetallic phases to form, such as binary phases (e.g. Mg2Si, Al2Cu),
ternary phases (e.g. β-Al5FeSi, Al2CuMg, AlFeMn, A17Cu4Ni and AlFeNi) and
quaternary phases (e.g. cubic α-Al15(FeMn)3Si2 and Al15Cu2Mg8Si6) [5, 6–10],
all of which may have some solubility for additional elements.
In AlSiCu cast alloy can form these intermetallic phases:
• Fe-rich intermetallic phases – Al5FeSi and Al15(FeMn)3Si2. The dominant
phase is phase know as beta- or β-needles phase Al5FeSi. This needle-shape
phase is more unwanted; because can bring high stress concentrations,
thereby increase crack imitation and decreasing the ductility [11, 12]. The
deleterious effect of Al5FeSi can be reduced by increasing the cooling rate
or superheating the molten metal. Another way that might by use to sup-
press the formation this monoclinic phase is converting the morphology by
the addition of a suitable “neutralizer” like Mn, Co, Cr, Ni, V, Mo and Be.
The most common addition has been Mn. Excess Mn may reduce Al5FeSi
phase and promote formation Fe-rich phases Al15(FeMn)3Si2 (know as
alpha- or α-phase) in form “skeleton like” or in form “Chinese script”.
This phase has according to some author’s cubic or hexagonal structure.
If Mg is also present with Si can phase called as pi- or π-phase form –
Al5Si6Mg8Fe2. Al5Si6Mg8Fe2 has script-like morphology [11–13].
THE STRUCTURE ANALYSIS OF SECONDARY (RECYCLED) ALSI9CU3. . . 199
• Cu-rich intermetallic phases – Al2Cu, Al-Al2Cu-Si and Al5Mg8Cu2Si6[11–14]. In unmodified alloys copper is present primarily as Al2Cu or Al-Al2Cu-Si phase, in modified alloys as Al5Mg8Cu2Si6. The average sizeof the copper phase decreases upon Sr modification. The Al2Cu phase isoften observed to precipitate both in a small blocky shape with microhard-ness 185 HV 0.01. Al-Al2Cu-Si phase is observed in very fine multi-phaseeutectic-like deposits with microhardness 280 HV 0.01 [5, 11, 14, 15].
Influence of intermetallic phases to mechanical and fatigue properties de-
pends on size, volume and morphology these phases [16]. The formation of these
phases should correspond to successive reactions during solidification with an
increasing number of phases involved at decreasing temperature. In practice,
Backerud et al. [17] identified five reactions in Al-Si-Cu alloy:
609◦C: α-dendritic network;
590◦C: Liq. → α-phase + Al15Mn3Si2 + Al5FeSi;
575◦C: Liq. → α-phase + Si + Al5FeSi;
525◦C: Liq. → α-phase + Al2Cu + Al5FeSi + Si;
507◦C: Liq. → α-phase + Al2Cu + Si + Al5Mg8Si6Cu2.
The quality and the tolerances of compositional secondary alloys are very
important, therefore are still under investigation of many academicals and indus-
trial projects. The purpose of the present article is to investigate microstructure
of cast Al-Si alloy (without and with heat treatment) prepared by recycling with
combination different analytical techniques (light microscopy upon black-white,
scanning electron microscopy (SEM) upon deep etching and energy dispersive
X-ray analysis (EDX)). As well as changes of the mechanical properties, which
are depending on the microstructure changes.
2. Experimental work
For investigation a microstructure was used the AlSi9Cu3 cast alloy with
phase. Nucleation of Si and Al2Cu may occur on large Al5FeSi platelets. Phase
with cubic crystal structure – Al15(FeMn)3Si2 is considered less harmful to the
mechanical properties than β phase [26, 27]. This phase (Fig. 5b) has a compact
morphology “Chinese script” or skeleton-like, which does not initiate cracks in
the cast material to the same extent as the Al5FeSi (Fig. 5a).
The Fe-rich particles can be twice as large as the Si particles, and the cool-
ing rate has a direct impact on the kinetics, quantities and size of Fe-rich in-
termetallic present in the microstructure. In experimental recycled AlSi9Cu3
cast alloy that contains less than 0.9% of Fe and 0.24% of Mn were observed
Al5FeSi needles (Fig. 5a) – on deep etcher samples plate-like form (Fig. 5a) and
Al15(FeMn)3Si2 – skeleton-like form (Fig. 5b). In experimental material was
satisfied condition Fe :Mn = 2 : 1, therefore intermetallic needles phases were
observed in a few isolated cases.
Heat treatment was use for affecting the size of Fe-rich phases, because the
shape and size of iron compounds is more influential than the quantity of those
iron compounds. The evolution of the Fe-rich phases during solution treatment
is described in Fig. 6. Al5FeSi phase is dissolved into very small needles (difficult
to observe). The Al15(MnFe)3Si2 phase was fragmented to smaller skeleton par-
ticles. In the untreated state Al15(FeMn)3Si2 phase has a compact skeleton-like
form (Fig. 5b). Solution treatment of this skeleton-like phase at 505◦C tends to
fragmentation (Fig. 6a) and at 515 or 525◦C to spheroidization and segmenta-
tion (Fig. 6b, c).
For the confirmation that solution treatment reduces Fe-rich phases area and
affects its morphology was used the quantitative metallography. Quantitative
metallography was carried out on an Image Analyzer NIS – Elements to quantify
Fe-rich phases (average area) morphology changes, during solution treatment.
Figure 6d shows the changes in the average area of Fe-rich phases during solution
treatment. The maximum average area of Fe-rich phases was observed in as-cast
samples (2 495 µm2). By increasing the solution temperature the average area
of Fe-phases drop to (the increasing temperature of solution treatment causes
dropping the average area of Fe-phases to 320 µm2 by 515◦C). With a prolonged
solution treatment time more than 8 h, the extent of dissolution of Fe-rich phases
changed little.
3.3. Cu-rich intermetallic phases
Half or more of the copper is found as a component of intermetallic com-
pounds [28]. Cu intermetallic phases are in aluminium alloys forming such as
Al2Cu with tetragonal crystal structure, which solidified in two morphologies
after Al-Si eutectic reaction. The first are as massive or blocky form (Al2Cu
THE STRUCTURE ANALYSIS OF SECONDARY (RECYCLED) ALSI9CU3. . . 209
– Fig. 7a-1, 7c) with high copper concentration ∼38–40 % Cu and second are
as fine ternary eutectic form (Al-Al2Cu-Si – Fig. 7a-2, 7b, 7d). The latter type
is more pronounced in the unmodified alloy and was observed either as sepa-
rate eutectic pockets or precipitated on pre-existing Si-particles or Fe-phases
[26, 28, 29]. In experimental material were observed both types of Cu-rich in-
termetallic phases (Fig. 7).
a) b)
c) d)
Fig. 7. Morphology of Cu-rich intermetallic phases in as-cast structure of AlSi9Cu3 cast alloy:a) 1-Al2Cu, 2- Al-Al2Cu-Si, etch. Dix-Keller, SEM, b) Al-Al2Cu-Si, deep etch. HCl, SEM,c) detail of Al2Cu phase, etch. Dix-Keller, d) detail of Al-Al2Cu-Si phase, etch. Dix-Keller.
The increasing level of Cu improves the strength of the aluminium alloythrough the formation of Cu based precipitate during heat treatment. The effectof heat treatment on morphology of Cu-rich phases was followed by optical and
THE STRUCTURE ANALYSIS OF SECONDARY (RECYCLED) ALSI9CU3. . . 211
electron microscopy. Morphology changes of Al-Al2Cu-Si during heat treatmentare demonstrated in Fig. 8. The changes of morphology of Al-Al2Cu-Si observedafter heat treatment are documented for holding time 4 hours.Al-Al2Cu-Si phase without heat treatment (as-cast state) occurs in form
compact oval troops (Fig. 7). After solution treatment at temperature 505◦Cthese phase disintegrated into smaller segments. The amount of Al-Al2Cu-Siphase decreases. This phase is gradually dissolved into the surrounding Al-matrix with an increase in solution treatment time (Fig. 8a). By solution treat-ment 515◦C was this phase observed in the form coarsened globular particles andthese occurs along the black needles, probably Fe-rich Al5FeSi phase (Fig. 8b).By solution treatment 525◦C was this phase documented in the form moltenparticles with homogenous shape (Fig. 8c).The changes of average area of Cu rich phases were confirmed by using the
quantitative metallography, too. Figure 8d shows average area of Cu-rich phasesobtained in solution heat treated samples. Maximum average area of Al-Al2Cu-Si phase was observed by temperature solution treatment at 505◦C with holdingtimes 2 hours (357µm2). Minimum average area of Al-Al2Cu-Si phase particlewas observed by temperature solution treatment at 515◦C (0.277 µm2). It isevident that heating at temperatures below the final solidification temperature(505◦C, 515◦C and 525◦C) results in dissolution of Al-Al2Cu-Si phase [29–31].Solution treatment at 525◦C apparently causes a marked change (Fig. 8). This,however, is attributed to the melting of the Al-Al2Cu-Si, rather than to itsdissolution. Dissolution and melting of Al2Cu phase in AlSi9Cu3 alloy has beenstudied in detail by Samuel [32]. When the AlSi9Cu3 alloy is solution treatedat temperature about the melting point of the eutectic (Al+Al2Cu) phase, e.g.525–540◦C, the Al-Al2Cu-Si particles may undergo incipient melting even afterperiods as 4 hours [29–31].
3.4. SEM image and X-ray analysis
The SEM image and X-rays analysis were used for a complete structuralanalysis of experimental material. Figure 9 shows typical example: a SEM imageand X-rays analysis of Al-Al2Cu-Si.Structural analysis identified of recycled (secondary) AlSi9Cu3 cast alloy
as basic structural elements: α-phase, Si platelets, Fe-rich intermetallic phases:needles – Al5FeSi (but in a small volume); skeleton-like Al15(FeMn)3Si2 phaseand Cu-rich intermetallic phase: Al2Cu (but in a small volume); Al-Al2Cu-Siternary eutectic. The EDX analysis revealed that the identified Cu-rich and Fe-rich intermetallic phases by using light microscopy are really these intermetallicphases, because chemical composition of these phases was confirmed by EDXanalysis.
212 L. HURTALOVA, E. TILLOVA, M. CHALUPOVA
a)
[Fig. 9]
THE STRUCTURE ANALYSIS OF SECONDARY (RECYCLED) ALSI9CU3. . . 213
b)
[Fig. 9]
214 L. HURTALOVA, E. TILLOVA, M. CHALUPOVA
c)
Fig. 9. Analysis of intermetallic phases in as-cast state of AlSi9Cu3 cast alloy, SEM:a) point X-ray analysis, b) line X-ray analysis, c) SEM image analysis.
3.5. Changes of mechanical properties causes with changes of structure
Heat treatment is one of the major factors used to enhance the mechanicalproperties of heat-treatable Al-Si alloys, through an optimization of both solu-tion and aging heat treatments. The solution treatment homogenises the caststructure and minimizes segregation of alloying elements in the casting. Seg-regation of solute elements resulting from dendritic solidification may have anadverse effect on mechanical properties.Changes of microstructural parameters cause changes in mechanical proper-
ties during solution treatment. Solution treatment performs tree roles: homog-enization of as-cast structure; dissolution of certain intermetallic phases suchas Al2Cu; changes the morphology of eutectic Si and intermetallic phases byfragmentation, spheroidization and coarsening, thereby improving mechanicalproperties.After heat treatment were samples subjected for mechanical test (strength
tensile and Brinell hardness). Influence of solution treatment and changes ofmicrostructural parameters on mechanical properties are shown on Fig. 10 and
THE STRUCTURE ANALYSIS OF SECONDARY (RECYCLED) ALSI9CU3. . . 215
Fig. 10. Changes of strength tensile.
Fig. 11. After solution treatment tensile strength and hardness are remarkablyimproved, compared to the corresponding as-cast condition. Highest strengthtensile was 273 MPa for 515◦C/4 hours (Fig. 10). With further increase in solu-tion temperature more than 515◦C and solution time more than 8 hours, tensilestrength gently decreases during the whole solution period.
Fig. 11. Changes of Brinell hardness.
Results of hardness (Fig. 11) are comparable with results of tensile strength.Highest hardness was 124 HBS for 515◦C/2 hours. The hardness decreases dur-ing the temperature 525◦C due to melting of the Al-Al2Cu-Si phase by thistemperature [29–31].
4. Conclusion
Understanding metal quality is of great importance for control and predictionof casting characteristics. The results of optical and SEM studies of recycled(secondary) AlSi9Cu3 cast alloy are summarized as follows:
• Structural analysis identified as basic structural elements: α-phase, Si platelets,and intermetallic phases (Al15(FeMn)3Si2 in the skeleton-like form, Al5FeSi
216 L. HURTALOVA, E. TILLOVA, M. CHALUPOVA
in form needles and Cu-ternary eutectic Al-Al2Cu-Si, Al2Cu in a small blockshape).
• In experimental material are dominant: Cu-rich phase Al-Al2Cu-Si and Fe-phases Al15(FeMn)3Si2 (thanks to the presence of Mn). Chemical compositionof all phases was confirmed by EDX analysis.
• During heat treatment Si particles spheroidized. As the optimum temperatureof spheroidization the eutectic Si was specified the temperature 515◦C.
• The morphology and size of iron phases are highly dependent on the solutiontreatment. Platelets Fe-rich phases (Al5FeSi) are dissolved into very smallneedle phases. Skeleton-like Fe-rich phases (Al15(FeMn)3Si2) are fragmentedand dissolved (average area reduces from 2 495 to 320 µm2).
• Al-Al2Cu-Si phases are fragmented, dissolved and redistributed within α-matrix (average area of Cu-phases particle decreases from 9 995.5 µm2 to0.277 µm2) during heat treatment.
• Changes of microstructural parameters of AlSi9Cu3 cause changes in mechan-ical properties. The highest strength tensile was at a temperature of 515◦Cwith holding time 4 hours; the highest hardness at a temperature of 515◦Cwith holding time 2 and 4 hours. For this was defined as optimum regime ofsolution treatment for experimental samples from AlSi9Cu3 cast alloy usingin automotive industries regime: 515◦C with a holding time of 4 hours, waterquenching at 40◦C and nature aging for 24 hours on air. After heat treat-ment, casts for automotive industries have better mechanical properties as inan as-cast state.
Acknowledgment
The authors acknowledge the financial support of the projects No. 1/0841/11and No. 1/0460/11.
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Received February 25, 2013; revised version June 24, 2013.